High Pressure NMR

High Pressure NMR Manifolds and Tubes Up To 2.5 kbar:



With an internal diameter of 3.0 mm these tubes have outstanding pressure tolerance and an impressure active volume.  Equal to about half that of a standard thin-walled 5 mm glass NMR tube these specialized tubes allow for high resolution triple-resonance spectroscopy to be performed on samples up to 2.5 kbar.  It is designed for use in standard high performance conventional or cryogenically cooled solution NMR probes.

The NMR cell connects to an external pressure source making possible changes to the internal pressure while inside the NMR.  Coupled with our Xtreme-60 Syringe Pump the system can provide automated maintenance or controlled pressure steps for your high pressure applications.   Cells with a valve integrated into the manifold are also available.  See the Reverse Micelle NMR section of this website for more details.

We offer a 2.0 kbar and 2.5 kbar rated version for Bruker and Varian.  Both are 5 mm O.D. x 3 mm I.D.

These tubes are very robust.  Unlike glass, quartz or sapphire they can withstand rough handling including drops off a bench without losing structural integrity.  Each tube is pressure certified by battery of tests at the factory.  The higher the pressure the more rigorous the tests performed.  Once certified the tubes can be repeatedly used in its matched manifold up to the certified pressure without failure. 

A manifold and tube is tested as single unit to assure optimal performance.  Each main component is identified by serial number to assure this continued pairing.  Documentation is also included for your records.   When matched units are listed on a quote the NMR cell unit is identified as BNC - X.X KBAR for Bruker and VNC - X.X. KBAR for Varian.


High Pressure NMR Cell (manifold & tube) specifications:

Wetted parts

7068 Aluminum, zirconia (NMR tube), Viton

Tube dimensions

Tube section: 5 mm O.D. x 3 mm I.D. x 87 mm length

Head section: 8 mm O.D. x 5 mm length

Tube volume

0.64 ml

Internal volume (manifold plus NMR tube)

Bruker: 0.81  ml

Varian: 0.76 ml

Temperature range

5°C - 100°C using standard seals

Pressure range

Indicated on certification sheet shipped with NMR tube

Manifold to tube seal

Viton seal standard; single-use

Pressure connection

Manifold port is HiP HF2 (1/2”-20 UNF) for use with 1/8” tubing.

Allowed fluids

All fluids compatible with the wetted parts can be used in the cell.  Examples are water, alcohols, alkanes, carbon dioxide, and xenon.  Some solvents may cause buildup of aluminum oxide on the NMR manifold. 

Cell assembly torque

130 in.-lbs. (14.7 Nm)         typical

160 in.-lbs. (18.1 Nm)         maximum

HM2 gland into manifold torque

72 in.-lbs (8.1 Nm)


Sales sheet for the high pressure NMR cell

User's manual for the high pressure NMR cell


Contact
sales@daedalusinnovations.com for quotes or other questions.

European customers contact David Cross at cross@rototec-spintec.com for quotes.





Xtreme-60 Syringe Pump:

Forget about using an HPLC pump to pressurize your samples.  Don't use a hand crank pump to try to maintain your quantitative pressure measurements over experiment times of days.

We are proud to offer the Xtreme-60 Syringe Pump for use in high pressure NMR applications.  It is capable of delivering and maintaining pressures up to 60,000 psi (4 kbar) without requiring user intervention.

Operation is simple: enter the set point and hit run.  The pump does the rest of the work.  Would you like to do a series of pressure points?  The Xtreme can be programmed for multi-point pressure titrations and data logging of the steps.

The Xtreme works with both liquids and gases.  Incompressible fluids such as water or light oils can be used as the pressurizing fluid without overstressing the pump drive train.

Xtreme-60 Specifications:

Power requirements

100-120 VAC / 200-240 VAC, 50/60 Hz

Power Cord

End-user supplied country compliant power cord with grounding terminal (except USA and Canada)

Input current

7.9 A / 3.95 A

Input fuse

10 A (GMA, 125V) / 5 A (GDB, 250V)

Power output

24 VDC, 20 A maximum

Output fuse

20 A (ABC, 250V)

Temperature range

10 °C to 70 °C

Weight

Main pump section: 109 lbs (49.5 kg)

Controller: 15 lbs (6.8 kg)

Dimensions

Main pump section: 12” W x 29” D x 11” H

Controller: 11” W x 17” D x 6” H

Pressure range

0-60,000 psi (4138 bar) maximum (US, Europe)

0-36,260 psi (2500 bar) maximum (Canada)

Wetted Parts

316 and 17-4PH stainless steel.  Parker Poly Pak® is standard.

Operating medium

Water, Oils, Alcohols, Inert Gases.  See Allowed Transducing Fluids in  manual for more details

System volume

12 ml (to internal valve)

12.5 ml with inlet valve closed and outlet valve open

Displacement volume

6.7 ml

Pressure connection

Inlet / Outlet ports are HiP HF4 (9/16”-18 UNF) for use with 1/4” tubing

Warm up time

5 minutes recommended from cold power-up

Normal operating temperature

15 °C to 40 °C

Resolution

0.01% FS (5 psi)

Pressure Sensor Specifications

Non-linearity: 0.35% FS

Hysteresis: 0.10% FS

Repeatability: 0.10% FS

Programmed pressure changes

100 steps (99999 minutes per step maximum)

Data acquisition

10000 data points

1-99999 second intervals

Maintenance of pressure setpoint

Indefinite

Full displacement

4 minutes at maximum speed

Standards met

UL 61010A-1, CSA C22.2 No. 61010-1, EN 61326-1:2006; Clause 7.2, EN 61326-1:2006; Table 2, EN 61010-1:2001

 

FCC, Class A, part 15, Canadian ICES-003 Class A


Sales sheet for the Xtreme-60 Syringe Pump

User's manual for the Xtreme-60 Syringe Pump


Contact sales@daedalusinnovations.com for quotes or other questions.

European customers contact David Cross at cross@rototec-spintec.com for quotes.




Support Equipment:


Safety Box:  This acrylic walled box provides protection to users while pressurizing cells.  It also helps protect the setup while moving samples from the bench to the spectrometer. It also provides a convenient place to store high pressure cells when not in use.  The box is open on the bottom.

Bruker and Varian versions are available.





Cell Setup Tool:  The high pressure tubes are not permanently fixed in the cell to allow for tubes to be switched and cleaned independently.  This benefit requires some care when assembling the high pressure cell.  This tool assists in that process by helping to keep the tube axially aligned with the cell during setup which improves seal integrity and lowers the probability of improper fit in the NMR.

Only one is needed for each cell type (Varian or Bruker) 





Other Cell Components:

High Pressure Seals (TS01):  These form the primary seal between the high pressure tube and manifold.  They are single use.  One version works for all tube and cell combinations.

 

 

Typical High Pressure Setup:

Listed below is the equipment that might be purchased for a high pressure setup for 45 samples up to 2.5 kbar pressure.

(1) Xtreme-60 Syringe Pump
(1) NMR Manifold plus 2.5 kbar tube (BNC - 2.5 KBAR or VNC - 2.5 KBAR)
(1) Cell Setup Tool
(1) Safety Box
(75) TS01 tube seals

The high pressure tubing and fittings required to connect to an external pressure source are not included with the cell since some customers already have such components.  However, we can add lengths of tubing to an order upon request.

It is possible to use the syringe pump for pressurizing multiple cells provided an external valve is added inline between the pump and the NMR tube.  This arrangement allows switching off between different samples and allows for storing of samples in the tube at modest pressures (i.e. ~0.5 kbar to slow any cell growth) between uses in the NMR. 

Contact sales@daedalusinnovations.com for quotes or other questions.

European customers contact David Cross at
cross@rototec-spintec.com for quotes.
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